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41.
以对苯二甲醛单缩醛与季戊四醇反应得到了2,4,8,10-四氧杂-2,9-二(4-二氰基乙烯基苯基)螺[5.5]十一烷(1), 经水解, 再与丙二腈反应, 制备了中间体2,4,8,10-四氧杂-2-(4-二氰基乙烯基苯基)-9-(4-甲酰基苯基)螺[5.5]十一烷(3). 8-(4-氧代环己烷基)-1,4-二氧杂螺[4.5]癸烷经芳构化形成2,6,10-三-(4-氧代环己烷基)-1,2,3,4,5,6,7,8,9,10,11,12-十二氢苯并[l]菲(4), 再与甲醛进行羟醛缩合, 制成了2,6,10-三-(4-羟基-3,3,5,5-四羟甲基环己烷基)-1,2,3,4,5,6,7,8,9,10,11,12-十二氢苯并[l]菲(5), 将5与过量的3反应, 得到了目标树形大分子化合物2,6,10-三-{15-(3,11-二(-4-(3-((9-(4-二氰基乙烯基)苯基)2,4,8,10-四氧杂螺[5.5]十一烷基)))-7-羟基-二螺[5.1.5.3]十六烷基)}-1,2,3,4,5,6,7,8,9,10,11,12-十二氢苯并[l]菲(6), 收率为18.1%. 产品结构经IR, 1H NMR, MS和元素分析进行了表征. 对影响反应的因素进行讨论. 相似文献
42.
A novel phosphorus-containing compound, poly(2-hydroxy propylene spirocyclic pentaerythritol bisphosphonate) (PPPBP) has been proved to be an excellent flame retardant for polyethylene terephthalate (PET) fabrics. In order to understand its flame retardant mode, FT-IR and XPS are used to investigate the char-forming mechanism of PPPBP. FT-IR spectra results show that with the increase of temperature, P-O-C group of PPPBP breaks down gradually, and species containing CC double bond appear. XPS spectra indicate that PPPBP produces phosphoric or polyphosphoric acid during thermo-decomposition. In the high temperature range (>400 °C), CC and phosphorus-containing complexes become the major components of the charred residue of PPPBP. Data of XPS and FT-IR spectra give positive evidence that PPPBP yields high amount of carbonaceous chars by producing phosphoric or polyphosphoric acid, which inhibit the oxidation of carbon atoms, and simultaneously impel the formation of carbon and species containing carbon double bond with outstanding heat resistance. 相似文献
43.
It is demonstrated that three kinds of neutral pentaerythritol derivatives possess promising host‐guest complexations with pillar[6]arenes both in solution and in the solid state. The inclusion structures were characterized by NMR spectroscopy and X‐ray crystallography. The complexation properties in different solvents were also investigated. 相似文献
44.
分别以硼酸、二乙醇胺、三氯氧磷和季戊四醇为原料,经酯化反应制得中间体二乙醇胺硼酸酯(DEAB, 1)和双季戊四醇二氯磷酸酯(SPDPC, 2); 1与2经缩聚反应合成新型集磷、氮、硼于一体的阻燃剂聚季戊四醇双磷酸酯二磷酰氯螺环二乙醇胺硼酸酯(PPSPSDB, 3),其结构经1H NMR, 13C NMR和FT-IR表征。考察了溶剂、物料比γ[n(2):n(1)]、反应温度和反应时间对3产率的影响,结果表明:在最佳反应条件(DMF为溶剂,γ=1 :1.2, 于120 ℃反应2 h后,于190 ℃反应2 h)下,产率93.26%。热重分析表明:3的初始分解温度为240.5 ℃, 800 ℃时残炭率为44.45%。 相似文献
45.
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47.
微波促进活性炭负载磷钨酸催化合成短链季戊四醇双缩醛 总被引:2,自引:0,他引:2
以活性炭负载磷钨酸为催化剂,用微波辐射法合成了5种短链季戊四醇双缩醛(3a~3 e),其中季戊四醇双缩丙醛(3b)未见文献报道。3的结构经1H NMR,IR和元素分析表征。 相似文献
48.
二代螺环树形化合物1,2,3,4,5,6,7,8,9,10,11,12-十二氢-2,2;6,6;10,10-三[3,3-二(烷氧羰基)-1,1-环亚丁基二甲氧基]三亚苯基的合成 总被引:1,自引:0,他引:1
以1,4-环己二酮、丙二酸二乙酯及多元醇等为原料, 经过两次“一锅煮”法合成了六种二代螺环树形化合物1,2,3,4,5,6,7,8,9,10,11,12-十二氢-2,2;6,6;10,10-三[3,3-二(烷氧羰基)-1,1-环亚丁基二甲氧基]三亚苯基螺环树形化合物, 其中烷氧基为异戊氧基、三羟甲基甲氧基、2,2-二溴甲基-3-羟丙氧基、2,2-二羟甲基丙氧基、二羟甲基膦甲氧基和(N-羟甲基-N-二羟甲基氨基乙基)甲氧基. 利用IR, NMR, MS和元素分析对合成的化合物进行了结构认证, 对影响反应的因素进行了讨论. 相似文献
49.
Due to being halogen‐free, non‐toxic, non‐erosive and environmentally friendly, melamine‐based flame retardants are attracting more and more attention. As a melamine‐based intumescent flame retardant, in this study the melamine salt of pentaerythritol phosphate (MPP) was prepared from melamine phosphate (MP) and pentaerythritol (PER). The reaction of MP with PER was then systematically investigated. The reaction product MPP was utilized to flame‐retard polypropylene (PP). FT‐IR, TGA and DSC were used to characterize MPP and also to investigate the reaction of MP and PER in depth. The experimental results show that MPP has good thermal stability and matched decomposition temperature with that of PP, making it suitable for flame retarding of PP. Also, MPP is melting‐blendable due to its softening during the heating process. The structure of MPP at a MP:PER molar ratio of 2.0 was confirmed as the same to that of the product synthesized from phosphorus oxychloride, pentaerythritol and melamine. The reaction of MP with PER was greatly influenced by the MP:PER proportion, reaction temperature and reaction time, rather than the physical state of PER, and the reaction mechanism of MP with PER was proposed. The prepared flame‐retarded polypropylene composite with 35 wt% intumescent flame‐retardant MPP has a flame retarding level of 3.2 mm UL 94 V‐0, tensile strength 27.0 MPa, Young's modulus 2442 MPa and Izod notched impact strength 3.8 kJ/m2. Copyright © 2007 John Wiley & Sons, Ltd. 相似文献
50.